反应详情

温度

60 °C

A mixture of 8-methyl-1H-quinolin-2-one (107) (580 mg, 3.6 mmol) and phosphorus oxychloride (5 mL) was stirred at 60° C. overnight. The mixture was then poured onto ice water and extracted with DCM (3×50 mL). The combined extracts were washed with water (2×100 mL) and dried with Na2SO4, and the solvent was removed. The residue was chromatographed on silica gel using 5% to 20% EtOAc in petroleum ether to give product (108) as small colorless crystals (400 mg, 2.3 mmol, 63% yield).

1. additionThe mixture was then poured onto ice water
2. extractionextracted with DCM (3×50 mL)
3. washThe combined extracts were washed with water (2×100 mL)
4. dry with materialdried with Na2SO4
5. customthe solvent was removed
6. customThe residue was chromatographed on silica gel using 5% to 20% EtOAc in petroleum ether